Dimethylformamide dimethyl acetal → (E)-6-(2,4-Difluorophenoxy)-2-(2-(dimethylamino)vinyl)nicotinonitrile

HRID 1620407ノート

反応式

HRID 1620407 の反応式
[F:1][C:2]1[CH:17]=[C:16]([F:18])[CH:15]=[CH:14][C:3]=1[O:4][C:5]1[CH:12]=[CH:11][C:8]([C:9]#[N:10])=[C:7]([CH3:13])[N:6]=1.CO[CH:21](OC)[N:22]([CH3:24])[CH3:23]>CN(C=O)C>[F:1][C:2]1[CH:17]=[C:16]([F:18])[CH:15]=[CH:14][C:3]=1[O:4][C:5]1[CH:12]=[CH:11][C:8]([C:9]#[N:10])=[C:7](/[CH:13]=[CH:21]/[N:22]([CH3:24])[CH3:23])[N:6]=1

参加物

4

反応物 2

HCID 78373Dimethylformamide dimethyl acetalHCID 674916176-(2,4-Difluorophenoxy)-2-methylnicotinonitrile

生成物 1

HCID 86664562(E)-6-(2,4-Difluorophenoxy)-2-(2-(dimethylamino)vinyl)nicotinonitrile

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 6-(2,4-difluorophenoxy)-2-methylnicotinonitrile (3.40 g, 14 mmol) in N,N-dimethylformamide dimethyl acetal (3.7 mL, 28 mmol) and DMF (5.00 mL) was heated at 140° C. in an oil bath for 18 h. The mixture was concentrated under reduced pressure to remove most of the DMF. The residue containing (E)-6-(2,4-difluorophenoxy)-2-(2-(dimethylamino)vinyl)nicotinonitrile (with some DMF) was used in the next step without further purification.

後処理

  1. concentrationThe mixture was concentrated under reduced pressure
  2. customto remove most of the DMF
  3. additionThe residue containing (E)-6-(2,4-difluorophenoxy)-2-(2-(dimethylamino)vinyl)nicotinonitrile (with some DMF)
  4. customwas used in the next step without further purification

出典と根拠

ORDレコード
ord-b025625f3c0747f6881bf5d401bf33ed
出典データセット
uspto-grants-2014_07
特許番号
US08772481B2

反応ノート

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